Intermediate phase asphalt raw material for producing carbon fibers and preparation method thereof
A technology of mesophase pitch and carbon fiber, which is applied in the fields of fiber chemical characteristics, textiles and papermaking, etc., can solve the problems of strong gas corrosion, low carbon fiber strength, increased production cost, etc., and achieves a simple and easy-to-control process and excellent pre-oxidation performance. , the effect of fast oxidation reaction
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Embodiment 1
[0024] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:5:0.5, react at 280°C for 120 minutes, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them. Then, the temperature of the reactor was raised to 350° C., nitrogen gas was continuously fed for 8 hours to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content used to measure the mesophase pitch is 100%, and S1 / S2 is 2.11 on the infrared absorption spectrogram, 13 The S3 / S4 on the C nuclear magnetic resonance spectrum is 3.76.
[0025] After the mesophase pitch was melt-spun at 320°C, the pitch fiber bundles were subjected to pre-oxidation treatment in the air atmosphere, and the temperature conditions were 5°C / min from room temperature to 100°C, and 0.5°C / min from 100°C To 300 ℃, keep at 300 ℃ for 20 minutes, the pre-oxidation performance of the pitch fiber is excellent, the mono...
Embodiment 2
[0027] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:10:0.5, react at 280°C for 120 minutes, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them. Then, the temperature of the reactor was raised to 350° C., nitrogen gas was continuously fed for 8 hours to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content used to measure the mesophase pitch is 100%, and S1 / S2 is 2.17 on the infrared absorption spectrogram, 13 S3 / S4 on the C nuclear magnetic resonance spectrum is 1.22.
[0028] After the mesophase pitch was melt-spun at 320°C, the pitch fiber bundles were subjected to pre-oxidation treatment in the air atmosphere, and the temperature conditions were 5°C / min from room temperature to 100°C, and 0.5°C / min from 100°C To 300 ℃, keep at 300 ℃ for 20 minutes, the pre-oxidation performance of the pitch fiber is excellent, the monofil...
Embodiment 3
[0030] Add methylnaphthalene, hydrogen fluoride and boron trifluoride compound into the reactor at a molar ratio of 1:15:0.5, react at 280°C for 120 minutes, discharge catalyst hydrogen fluoride and fluorine triboride and recycle them. Then, the temperature of the reactor was raised to 350° C., nitrogen gas was continuously fed for 8 hours to remove low-boiling point products, and the temperature was lowered to obtain mesophase pitch. The mesophase content used to measure the mesophase pitch is 100%, and S1 / S2 is 2.29 on the infrared absorption spectrogram, 13 The S3 / S4 on the C nuclear magnetic resonance spectrum is 1.04.
[0031] After the mesophase pitch was melt-spun at 320°C, the pitch fiber bundles were subjected to pre-oxidation treatment in the air atmosphere, and the temperature conditions were 5°C / min from room temperature to 100°C, and 0.5°C / min from 100°C To 300 ℃, keep at 300 ℃ for 20 minutes, the pre-oxidation performance of the pitch fiber is excellent, the mon...
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